CN105585194B - One kind contains Na+、K+、NH4+、Cl‑、SO42‑、NO3‑The highly concentrated effluent brine method of comprehensive utilization of coal chemical industry - Google Patents

One kind contains Na+、K+、NH4+、Cl‑、SO42‑、NO3‑The highly concentrated effluent brine method of comprehensive utilization of coal chemical industry Download PDF

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CN105585194B
CN105585194B CN201610008828.0A CN201610008828A CN105585194B CN 105585194 B CN105585194 B CN 105585194B CN 201610008828 A CN201610008828 A CN 201610008828A CN 105585194 B CN105585194 B CN 105585194B
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water
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sodium chloride
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CN105585194A (en
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王文领
秦晓丽
屈剑
吴玄斌
张灵
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王文领
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water, or sewage
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/04Chlorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00Sulfates or sulfites of sodium, potassium or alkali metals in general
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C3/00Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00General aspects of water treatment
    • C02F2301/08Multistage treatments, e.g. repetition of the same process step under different conditions
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F5/00Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
    • C02F5/02Softening water by precipitation of the hardness
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

The present invention relates to one kind to contain Na+、Ka+、NH4 +、Cl、SO4 2‑、NO3 The highly concentrated effluent brine method of comprehensive utilization of coal chemical industry, after the softened removal of impurities of highly concentrated effluent brine, coagulating sedimentation remove COD, its water is concentrated 20 30% by aerial cooler;Two level, three-level concentration systems and salt-mixture recovery system are entered back into, using the method for multiple-effect negative pressure evaporation, concentrating and separating sodium sulphate, sodium chloride and sodium nitrate, potassium sulfate salt-mixture;Recycling condensing water.Sodium chloride, the sodium sulphate high purity more than 99% isolated, directly can externally sell.The present invention has significant economic benefit and social benefit, and realizes environmentally friendly overall up to standard, it can also be used to which other industry utilizes similar to the integrated treatment of high concentration salt solution.So as to reach the environmental protection and energy saving requirement of resource full utilization.

Description

One kind contains Na+、K+、NH4+、Cl-、SO42-、NO3-Coal chemical industry highly concentrated effluent brine synthesis profit Use method
Technical field
The invention belongs to the wastewater treatment link of the chemical fields such as coal chemical industry, new energy chemical industry, petrochemical industry, chemical fertilizer, tool Body is related to containing Na+、K+、NH4 +、Cl-、SO4 2-、NO3 -Coal chemical industry highly concentrated effluent brine in-depth processing and method of comprehensive utilization.
Background technology
The emerging energies such as coal chemical industry, methanol, ethylene glycol, alkene and chemical industry, fertilizer enterprises are in wastewater deepening processing and reuse During, by Sewage Disposal waste water up to standard, the dense draining of Desultwater Station, circulate water station the waste water such as sewer mix after, it is unified Purified treatment is carried out by waste water discharge-reducing device, purified water therein returns to be recycled in production process, shape after purified treatment Na is rich in into a small amount of+、K+、NH4 +、Cl-、SO4 2-、NO3 -The high concentration salt solution of plasma, referred to as highly concentrated effluent brine.Its is main Composition composition is as shown in the table:
Component target Unit Influent quality
Sodium mg/L 20000-35000
Potassium mg/L 400-800
Basicity Mg/L is (with CaCO3Meter) 1500-2500
Chlorion mg/L 10000-20000
Sulfate radical mg/L 8000-20000
Nitrate anion mg/L 2500-4000
Silica mg/L 400-800
COD mg/L 600-1000
Ammonium mg/L 100-250
pH 10-11.5
It is total molten solid mg/L 40000-65000
Due to containing higher inorganic salts and ammonia nitrogen in the highly concentrated effluent brine in this part, COD is also higher, can not directly discharge, Can not directly it utilize.Indivedual enterprises are concentrated using the method for single vaporization concentration, but concentrate inorganic salts mixing out Together, and colourity, outward appearance are poor, can not utilize, can not also handle, turn into secondary pollution, be punished by environmental administration.For This, tries to explore new processing method and processing unit, on the premise of national environmental standard is met, by this part hc effluent Comprehensive utilization of resources is carried out, turns into the important and eager task of above-mentioned enterprise and scientific research institution.
Therefore, coal chemical industry enterprises and methanol, alkene, emerging energy enterprise and chemical industry, fertilizer enterprises, are badly in need of a kind of method energy Caused highly concentrated effluent brine in wastewater deepening processing procedure is comprehensively utilized, realizes the environmental objective of wastewater zero discharge;Together When invest rather moderate, operating cost is relatively low.Only in this way, the long-term health development of Chemical Industry could be ensured.
The content of the invention
It is an object of the invention to provide one kind to contain Na+、K+、NH4 +、Cl-、SO4 2-、NO3 -Coal chemical industry highly concentrated effluent brine synthesis Application way, making highly concentrated effluent brine, inorganic salts therein can be utilized respectively after processing, the waste water recycling enterprise life after processing Production system, is fully achieved national requirements for environmental protection, so as to turn waste into wealth, realizes comprehensive utilization of resources, finally improves the quality of production, carry Rise social and economic benefit.
To achieve the above object, the scheme that uses of the present invention is:One kind contains Na+、K+、NH4 +、Cl-、SO4 2-、 NO3 -Coal The highly concentrated effluent brine method of comprehensive utilization of chemical industry, comprises the steps:
(1) hardness is removed:It is clear that pH value 10.5-11 highly concentrated effluent brine (abbreviation high-salt wastewater, similarly hereinafter) is pumped into softening first Clear pond, the liquid caustic soda for adding mass concentration 42-50% adjust pH value to 11.5-12, make the Mg in waste water2+With the shape of magnesium hydroxide Formula precipitates;Then sodium carbonate is added, by Ca in water2+Content, add 1-1.5 kilograms per square waste water, purity is more than 98%, Make Ca2+Precipitate as calcium carbonate;To make precipitation abundant, the speed that agitator is turned by 50-60 per minute in pond is slow Stirring;During magnesium hydrate precipitate, silica can precipitate a part therewith, so as to reduce the concentration of silica in water;Pass through Pulp pump, from depositing reservoir bottom collection precipitating sludge is softened, is discharged into the existing sludge collecting pit of enterprise at interval of 48-72 hours, Mixed with original sludge;Mixing sludge is dehydrated to solid content in 30-40% through centrifugal dehydrator, by transported on trucks to sludge Reason factory and office put;
(2) one-level coagulating sedimentation tentatively removes COD:To remove up to 600-1000mg/L COD in highly concentrated effluent brine, The technique of acid coagulation is taken to be degraded:Softening depositing reservoir supernatant overflow enters one-level coagulative precipitation tank, passes through acid adding meter Mass concentration 25-31% hydrochloric acid is continuously added in pond and stirred by amount pump, and pH value is adjusted to 2-3, makes to remain in supernatant Calcium, magnesium ion is dissolved into water in the form of calcium chloride, magnesium chloride;Coagulation occurs for Organic substance in water simultaneously, adds polyaluminium Ferric flocculant, per square 20-50 grams of waste water dosage, further flocculation sediment is allowed to, the organic particle to precipitate is through Pulp pump The existing sludge collecting pit of enterprise is squeezed at interval of 48-72 hours, with original sludge mixed processing;The supernatant overflowed Filter to be squeezed into through pump to be filtered, the high-salt wastewater after filtering enters high-salt wastewater primary concentration system buffer pool by overbottom pressure, The impurity filtered out is periodically discharged into the existing sludge collecting pit of enterprise;COD contents are down to 350- after one-level coagulating sedimentation 450mg/L;
(3) high-salt wastewater primary concentration:The liquid caustic soda that mass concentration 42-50% is added into buffer pool adjusts waste water pH value Section squeezes into primary concentration system air cooler to 6.5-7, then boosted pump, is flowed from top to bottom after cloth liquid;It is outside empty Gas introduces aerial cooler through air blower, is flowed from bottom to top through subcooler inner stuffing;Air-liquid two-phase adverse current between filler Contact, the clean moisture in high-salt wastewater constantly evaporates to be shifted into air, therein when air is reached at the top of aerial cooler Vapor reaches saturation partial pressure, mass concentration 15-20% moisture air inlet in the form of saturated steam in high-salt wastewater In, unsaturated air is changed into saturated air, after aerial cooler epimere dehydrater further removes aqueous water, from top It is discharged into air, high-salt wastewater is obtained initial concentration, so as to saves the cost of later stage concentration;By the high-salt wastewater of initial concentration Again it is discharged into primary concentration system buffer pool, carries out circulation concentration;
(4) high-salt wastewater secondary concentration:The high-salt wastewater for obtaining initial concentration squeezes into waste water two level through pump from buffer pool The evaporator of concentration systems, by the way of multiple-effect evaporation concentration, heated with external 0.4-0.6MPa low pressure saturated steam, 55-120 DEG C, by Waste water concentrating to sodium chloride therein close to saturation;Evaporation condensed water and water vapor condensation water are from secondary concentration System is discharged, and respectively enters evaporative condenser water pot and steam condensate (SC) tank is standby;Concentrated mother liquor is discharged into two-stage coagulation sedimentation basin;
(5) two-stage coagulation precipitation removes COD again:In high-salt wastewater after I and II concentrates, the concentration of COD contents To 6000-6500mg/L, the technique of secondary acid coagulation is taken further to degrade:High-salt wastewater concentrated mother liquor after secondary concentration Two-stage coagulation sedimentation basin is pumped into, continuously mass concentration 25-31% hydrochloric acid is added in pond and stirred by acid adding measuring pump, PH value is adjusted to 2-3, makes the Ca remained in mother liquor2+、Mg2+Ion is dissolved into water in the form of calcium chloride, magnesium chloride;Together When Organic substance in water, coagulation occurs, adds poly ferric chloride flocculant agent, per square 20-50 grams of waste water dosage, it is heavy to be allowed to further flocculation Form sediment, the organic particle to precipitate squeezes into the existing sludge collecting pit of enterprise through Pulp pump at interval of 48-72 hours, and original Sludge mixed processing;The supernatant overflowed is squeezed into filter through pump and filtered;Mother liquor after filtering is squeezed into plus alkali pond, The liquid caustic soda for adding mass concentration 42-50% adjusts pH value to 6-7, and the supernatant overflowed squeezes into filter mistake again through pump Filter;High-salt wastewater after secondary filter enters high-salt wastewater three-level concentration systems by overbottom pressure;Two-stage coagulation sedimentation basin plus alkali bottom of pond Portion's mud and the impurity filtered out are periodically discharged into the existing sludge collecting pit of enterprise;The COD contents after two-stage coagulation precipitates It is down to 1000-1500mg/L;
(6) waste water three-level concentration and recovery anhydrous sodium sulfate:Salt-mixture mother liquor after two-stage coagulation precipitates and filters, through pump Waste water three-level concentration systems evaporator is squeezed into, takes the mode of evaporation and concentration, between 70-75 DEG C, by Waste water concentrating to therein Potassium sulfate is close to saturation, so that the sodium chloride, sodium sulphate mass crystallization in waste water separate out, through further stiff, into centrifugation Machine carries out first-stage centrifugal separation;Sodium sulphate, the sodium chloride mixture isolated add the evaporation condensed water of secondary concentration system, 70-75 DEG C sodium chloride therein is completely dissolved after carry out two-stage centrifugal separation;It is dense that the sodium sulphate centrifuged out adds two level The evaporation condensed water of compression system, is washed at 70-75 DEG C, and sodium chloride therein is completely dissolved, and then carries out three-level centrifugation Separation, obtains the anhydrous sodium sulfate of high-purity, and entering warehouse after the processing of dry packing system sell;The mother liquor of first-stage centrifugal separation Salt-mixture system for concentrating and recycling is pumped into, the mother liquor of two-stage centrifugal separation is pumped into sodium chloride, sulfuric acid mother liquid of sodium freezing and crystallizing system;Three Level centrifuges cleaning solution and squeezes into sal glauberi evaporator;Three-level concentration does heat using indirect steam caused by secondary concentration Source, outer next life steam is not consumed, it is standby that evaporation condensed water is discharged into evaporative condenser water pot;
(7) sodium chloride, sulfuric acid mother liquid of sodium freezing and crystallizing reclaim sodium sulphate again:Waste water three-level concentration systems two-stage centrifugal point From sodium chloride, sulfuric acid mother liquid of sodium frozen cooling to -5-0 DEG C, sal glauberi mass crystallization separates out, after first-stage centrifugal separation, Evaporation condensed water dissolving is added, and three-level concentration systems are drained through the three-level centrifugation sodium sulphate cleaning solution come and enter ten water together Sodium sulphate evaporator, thermal source is done using indirect steam caused by secondary concentration, concentration, anhydrous slufuric acid are evaporated at 70-75 DEG C Sodium mass crystallization is separated out, and two-stage centrifugal separation is carried out into centrifuge;Solid sodium sulfate after centrifugation is sent into three-level concentration System, and the sodium sulphate that three-level concentration systems two-stage centrifugal is separated wash recovery in the lump;After sal glauberi centrifuges Mother liquor be pumped into salt-mixture system for concentrating and recycling;It is standby that evaporation condensed water is discharged into evaporative condenser water pot;Reclaimed through step (6)-(7) Sodium sulphate mixing after, by mass percentage, sodium sulphate purity 98-99.13%, the rate of recovery be more than 98%, sodium chloride content is not More than 1%, nitric acid sodium content is no more than 0.4%, and sulfuric acid potassium content is no more than 0.1%;
(8) sodium chloride mother liquor concentrations recovery sodium chloride:Sal glauberi centrifuges mother liquor and is pumped into sodium chloride evaporator, leans on 0.4-0.6MPa external vapor heat supply, solution being evaporated to supersaturation at 100-120 DEG C, sodium chloride mass crystallization separates out, Through stiff, first-stage centrifugal separation is carried out into centrifuge;The evaporation that the sodium chloride centrifuged out adds secondary concentration system is cold Condensate, washed at 70-75 DEG C, sodium sulphate therein, potassium sulfate, sodium nitrate are completely dissolved, then carry out two-stage centrifugal Separation, obtains the sodium chloride of high-purity, and entering warehouse after the processing of dry packing system sell;One-level, the mother of two-stage centrifugal separation After liquid mixing, mass concentration 80-85% squeezes into sodium chloride, the water sulphur of sulfuric acid mother liquid of sodium freezing and crystallizing system circulation freezing and crystallizing ten Sour sodium, mass concentration 15-20% are pumped into salt-mixture system for concentrating and recycling;It is standby that steam condensate (SC) is discharged into steam condensate (SC) tank;Return In the sodium chloride of receipts, by mass percentage, sodium chloride purity 98-99.13%, rate of recovery 88-90.77%, sodium sulphate content is not More than 0.5%, nitric acid sodium content is no more than 0.5%, and sulfuric acid potassium content is no more than 0.2%;
(9) salt-mixture concentration and recovery:Mother liquor, ten water sulfuric acid after the separation of waste water three-level concentration systems sodium sulphate first-stage centrifugal Mother liquor after sodium evaporator evaporation and two-stage centrifugal separation, after being mixed into salt-mixture concentration systems, it is pumped into salt-mixture concentration system System is evaporated concentration, and thermal source, between 60-90 DEG C, 3K are used as by the use of the indirect steam of sodium chloride system for concentrating and recycling2SO4· Na2SO4、NaNO3·Na2SO4、NaNO3、(NH4)2SO4Salt-mixture mass crystallization separates out, and is centrifuged through stiff into centrifuge Separation;The solid salt-mixture moisture content mass percent centrifuged out be no more than 5%, it is packaged after directly as agricultural mixing Chemical fertilizer is sold;Mass concentration 80-85% mother liquors after centrifugation squeeze into the crystallization of salt-mixture system for concentrating and recycling circulating and evaporating, matter Amount concentration 15-20% squeezes into the original sludge treatment pond of enterprise, is handled together with other impurities sludge;Evaporation condensed water is discharged into steaming It is standby to send out condensate water pot;The salt-mixture of recovery, by mass percentage, nitric acid sodium content 50-60.03%, potassium sulfate contain in butt 15.5-20.55% is measured, sodium sulphate content is no more than 5%, ammonium sulphate content 8.3-12.1%, sodium chloride content 5.7-9.47%, Other impurities are no more than 4%;
(10) recovered steam condensed water and evaporation condensed water:The remaining evaporation condensed water of evaporative condenser water pot is straight by enterprise Take back and use production system, rate of recovery 90-93%;Residual steam condensed water is by enterprise's direct reuse steam generator system, rate of recovery 95- 97%.
High-salt wastewater passes through above-mentioned steps (1)-(10), and sodium chloride therein, sodium sulphate are separately recovered, sodium nitrate, sulphur Sour potassium is reclaimed in the form of salt-mixture, is used directly as agrochemical, reuse production system after waste water is evaporated, so as to reach The environmental protection that is recycled completely to resource, power conservation requirement.
The main characteristic of the invention lies in that:(1) solubility using sodium chloride, sodium sulphate, sodium nitrate, potassium sulfate when molten altogether Difference, it is separated respectively;(2) initial concentration is carried out to high-salt wastewater using aerial cooler, it is negative reduces waste water evaporation Lotus and steam consumption quantity;(3) secondary concentration is carried out to waste water using the waste water of multiple-effect evaporation, further reduces steam consumption quantity;(4) adopt Impurities in water and COD are removed with Wastewater Pretreatment and the method for coagulating sedimentation, improves product purity;The sodium chloride (5) isolated, Sodium sulphate high purity more than 99%, directly can externally it sell.The present invention has significant economic benefit and social benefit, and in fact Existing environmentally friendly overall up to standard, it can also be used to which other industry utilizes similar to the integrated treatment of high concentration salt solution.
Brief description of the drawings
Fig. 1 is present invention process schematic flow sheet.
Embodiment:
One kind contains Na+、K+、NH4 +、Cl-、SO4 2-、NO3 -The highly concentrated effluent brine method of comprehensive utilization of coal chemical industry, it is including following Step:
(1) hardness is removed.PH value 10.5-11 highly concentrated effluent brine (abbreviation high-salt wastewater, similarly hereinafter) is pumped into the system first Soften depositing reservoir, the liquid caustic soda for adding 42-50% (mass concentration, similarly hereinafter) adjusts pH value to 11.5-12, makes the Mg in waste water2+ Precipitated in the form of magnesium hydroxide;Then a small amount of sodium carbonate is added, by Ca in water2+Content, add 1-1.5 per square waste water Kilogram, purity is more than 98%, makes Ca2+Precipitate as calcium carbonate;To make precipitation abundant, agitator is by per minute in pond 60 turns of speed is slowly stirred;During magnesium hydrate precipitate, silica can precipitate a part therewith, so as to reduce titanium dioxide in water The concentration of silicon;The existing dirt of enterprise was discharged into from softening depositing reservoir bottom collection precipitating sludge at interval of 48 hours by Pulp pump Mud collecting pit, mixed with original sludge;Mixing sludge is dehydrated to solid content in 30-40% through centrifugal dehydrator, is transported by truck Treatment of Sludge factory and office are delivered to put;
(2) one-level coagulating sedimentation tentatively removes COD.To remove up to 800mg/L COD in highly concentrated effluent brine, acid is taken The technique of property coagulation is degraded.Softening depositing reservoir supernatant overflow enters one-level coagulative precipitation tank, is connected by acid adding measuring pump The continuous hydrochloric acid by mass concentration 31% (mass concentration, similarly hereinafter) is added in pond and stirred, and pH value is adjusted to 2-3, makes supernatant Calcium, the magnesium ion of middle residual are dissolved into water in the form of calcium chloride, magnesium chloride;Coagulation, addition polymerization occur for Organic substance in water simultaneously Chlorination ferric flocculant is closed, per square 20-50 grams of waste water dosage, is allowed to further flocculation sediment, the organic particle warp to precipitate Pulp pump squeezed into the existing sludge collecting pit of enterprise at interval of 48 hours, with original sludge mixed processing;What is overflowed is upper Clear liquid is squeezed into filter through pump and filtered, and the high-salt wastewater after filtering enters high-salt wastewater primary concentration system buffer by overbottom pressure Pond, the impurity filtered out are periodically discharged into the existing sludge collecting pit of enterprise;COD contents are down to after one-level coagulating sedimentation 350-450mg/L;
(3) high-salt wastewater primary concentration.The liquid caustic soda that 42-50% is added into buffer pool adjusts pH value of waste water to 6.5-7, Then boosted pump squeezes into primary concentration system air cooler, is flowed from top to bottom after cloth liquid;Extraneous air is through air blower Aerial cooler is introduced, is flowed from bottom to top through subcooler inner stuffing;Air-liquid two-phase counter current contacting between filler, high salt Clean moisture in waste water constantly evaporates to be shifted into air, and when air is reached at the top of aerial cooler, vapor therein reaches To saturation partial pressure, 15-20% moisture is got into the air in the form of saturated steam in high-salt wastewater, becomes unsaturated air For saturated air, after aerial cooler epimere dehydrater further removes aqueous water, it is discharged into from top in air, makes high salt Waste water obtains initial concentration, so as to save the cost of later stage concentration;Primary concentration is discharged into by the high-salt wastewater of initial concentration again In system buffer pool, circulation concentration is carried out;
(4) high-salt wastewater secondary concentration.The high-salt wastewater for obtaining initial concentration squeezes into waste water two level through pump from buffer pool The evaporator of concentration systems, by the way of multiple-effect evaporation concentration, added with external Low pressure steam (0.6MPa saturated vapors) Heat, at 55-120 DEG C, by Waste water concentrating to sodium chloride therein close to saturation;Evaporation condensed water and water vapor condensation water are from two level Concentration systems are discharged, and respectively enter evaporative condenser water pot and steam condensate (SC) tank is standby;Concentrated mother liquor is discharged into two-stage coagulation precipitation Pond;
(5) two-stage coagulation precipitation removes COD again.In high-salt wastewater after I and II concentrates, the concentration of COD contents To 6000-6500mg/L, the technique of secondary acid coagulation is taken further to degrade.High-salt wastewater concentrated mother liquor after secondary concentration Two-stage coagulation sedimentation basin is pumped into, continuously the hydrochloric acid of mass concentration 31% is added in pond and stirred by acid adding measuring pump, by pH Value regulation makes the Ca remained in mother liquor to 2-32+、Mg2+Ion is dissolved into water in the form of calcium chloride, magnesium chloride;Water simultaneously Middle organic matter, coagulation occurs, adds poly ferric chloride flocculant agent, per square 20-50 grams of waste water dosage, be allowed to further flocculation sediment, The organic particle to precipitate squeezed into the existing sludge collecting pit of enterprise through Pulp pump at interval of 48 hours, with original sludge Mixed processing;The supernatant overflowed is squeezed into filter through pump and filtered;Mother liquor after filtering is squeezed into plus alkali pond, adds 42-50% liquid caustic soda adjusts pH value to 6-7, and the supernatant overflowed is squeezed into filter through pump and filtered again;Secondary filter High-salt wastewater afterwards enters high-salt wastewater three-level concentration systems by overbottom pressure;Coagulating basin, add alkali bottom of pond portion's mud and filter out Impurity be periodically discharged into the existing sludge collecting pit of enterprise;COD contents are down to 1000-1500mg/L after two-stage coagulation precipitates;
(6) waste water three-level concentration and recovery anhydrous sodium sulfate.Salt-mixture mother liquor after two-stage coagulation precipitates and filters, through pump Waste water three-level concentration systems evaporator is squeezed into, takes the mode of evaporation and concentration, between 70-75 DEG C, by Waste water concentrating to therein Potassium sulfate is close to saturation, so that the sodium chloride, sodium sulphate mass crystallization in waste water separate out, through further stiff, into centrifugation Machine carries out first-stage centrifugal separation;Sodium sulphate, the sodium chloride mixture isolated add the evaporation condensed water of secondary concentration system, 70-75 DEG C sodium chloride therein is completely dissolved after carry out two-stage centrifugal separation;It is dense that the sodium sulphate centrifuged out adds two level The evaporation condensed water of compression system, is washed at 70-75 DEG C, and sodium chloride therein is completely dissolved, and then carries out three-level centrifugation Separation, obtains the anhydrous sodium sulfate of high-purity, and entering warehouse after the processing of dry packing system sell;The mother liquor of first-stage centrifugal separation Salt-mixture system for concentrating and recycling is pumped into, the mother liquor of two-stage centrifugal separation is pumped into sodium chloride, sulfuric acid mother liquid of sodium freezing and crystallizing system;Three Level centrifuges mother liquor and squeezes into sal glauberi evaporator;Three-level concentration does thermal source using indirect steam caused by secondary concentration, Outer next life steam is not consumed, and it is standby that evaporation condensed water is discharged into evaporative condenser water pot;
(7) sodium chloride, sulfuric acid mother liquid of sodium freezing and crystallizing reclaim sodium sulphate again.Waste water three-level concentration systems two-stage centrifugal point From sodium chloride, sulfuric acid mother liquid of sodium frozen cooling to -5-0 DEG C, sal glauberi mass crystallization separates out, after first-stage centrifugal separation, Evaporation condensed water dissolving is added, and three-level concentration systems are drained through the three-level centrifugation mother liquor (sodium sulphate cleaning solution) come and entered together Enter sal glauberi evaporator, thermal source is done using indirect steam caused by secondary concentration, concentration, nothing are evaporated at 70-75 DEG C Aqueous sodium persulfate mass crystallization is separated out, and two-stage centrifugal separation is carried out into centrifuge;Solid sodium sulfate after centrifugation is sent into three Level concentration systems, and the sodium sulphate that three-level concentration systems two-stage centrifugal is separated wash recovery in the lump;Sal glauberi centrifuges Mother liquor after separation is pumped into salt-mixture system for concentrating and recycling;It is standby that evaporation condensed water is discharged into evaporative condenser water pot;Through step (6)- (7) after the sodium sulphate mixing of recovery, by mass percentage, sodium sulphate purity 98-99.13%, the rate of recovery is more than 98%, sodium chloride Content is no more than 1%, and nitric acid sodium content is no more than 0.4%, and sulfuric acid potassium content is no more than 0.1%;
(8) sodium chloride mother liquor concentrations recovery sodium chloride.Sal glauberi centrifuges mother liquor and is pumped into the steaming of the system sodium chloride Device is sent out, by 0.6MPa external vapor heat supply, solution is evaporated to supersaturation, the analysis of sodium chloride mass crystallization at 100-120 DEG C Go out, through stiff, first-stage centrifugal separation is carried out into centrifuge;The sodium chloride centrifuged out adds the evaporation of secondary concentration system Condensed water, washed at 70-75 DEG C, sodium sulphate therein, potassium sulfate, sodium nitrate be completely dissolved, then carry out two level from The heart separates, and obtains the sodium chloride of high-purity, and entering warehouse after the processing of dry packing system sell;One-level, two-stage centrifugal separate After mother liquor mixing, wherein the 80-85% of mixing mother liquor mass flow squeezes into sodium chloride, sulfuric acid mother liquid of sodium freezing and crystallizing system circulation Freezing and crystallizing sal glauberi, the 15-20% of mixing mother liquor mass flow are pumped into salt-mixture system for concentrating and recycling;Steam condensate (SC) It is standby to be discharged into steam condensate (SC) tank;In the sodium chloride of recovery, by mass percentage, sodium chloride purity 98-99.13%, the rate of recovery 88-90.77%, sodium sulphate content are no more than 0.5%, and nitric acid sodium content is no more than 0.5%, and sulfuric acid potassium content is no more than 0.2%;
(9) salt-mixture concentration and recovery.Mother liquor, ten water sulfuric acid after the separation of waste water three-level concentration systems sodium sulphate first-stage centrifugal Mother liquor after sodium evaporator evaporation and two-stage centrifugal separation, after being mixed into salt-mixture concentration systems, it is pumped into salt-mixture concentration system System is evaporated concentration, and thermal source, between 60-90 DEG C, salt-mixture are used as by the use of the indirect steam of sodium chloride system for concentrating and recycling (3K2SO4·Na2SO4、NaNO3·Na2SO4、NaNO3、(NH4)2SO4) mass crystallization precipitation, carried out through stiff into centrifuge Centrifuge;The solid salt-mixture moisture content centrifuged out is no more than 5% (mass percent), it is packaged after directly as agriculture Sold with mixed fertilizer;Mother liquor 80-85% after centrifugation squeezes into the crystallization of evaporator circulating and evaporating, and 15-20% squeezes into enterprise Original sludge treatment pond, handled together with other impurities sludge;It is standby that evaporation condensed water is discharged into evaporative condenser water pot;Recovery Salt-mixture, by mass percentage, nitric acid sodium content 50-60.03% in butt, sulfuric acid potassium content 15.5-20.55%, sodium sulphate Content is no more than 5%, and ammonium sulphate content 8.3-12.1%, sodium chloride content 5.7-9.47%, other impurities are no more than 4%;
(10) recovered steam condensed water and evaporation condensed water.The remaining evaporation condensed water of evaporative condenser water pot is straight by enterprise Take back and use production system, rate of recovery 90-93%;Residual steam condensed water is by enterprise's direct reuse steam generator system, rate of recovery 95- 97%.
High-salt wastewater passes through above-mentioned steps (1)-(10), and sodium chloride therein, sodium sulphate are separately recovered, sodium nitrate, sulphur Sour potassium is reclaimed in the form of salt-mixture, is used directly as agrochemical, reuse production system after waste water is evaporated, so as to reach The environmental protection that is recycled completely to resource, power conservation requirement.
Capital equipment of the present invention, facility include:
1st, high-salt wastewater pretreatment system:By softening depositing reservoir, one-level, two-stage coagulation sedimentation basin plus alkali pond, waste water lifting The key facilities such as pump, filter, equipment composition;
2nd, high-salt wastewater primary concentration system:It is made up of buffer pool, aerial cooler, air blower, elevator pump etc.;
3rd, high-salt wastewater secondary concentration system:It is made up of heater, evaporator, circulating pump, vavuum pump, condensate water pot etc.;
4th, high-salt wastewater three-level concentration systems:By heater, evaporator, circulating pump, thickener, crystallizer, centrifuge etc. Composition;
5th, sodium chloride, sodium sulphate separation and recovery system:Including dissolving tank, washer, centrifuge, heater, evaporator, thick Thick device, crystallizer, refrigeration system, circulating pump, drying machine, packing machine etc. form;
6th, salt-mixture recovery system:It is made up of heater, evaporator, thickener, crystallizer, centrifuge, circulating pump etc.;
7th, electric, blind controller system:It is made up of electrical system, DCS control systems and control valve, control instrument etc..
In apparatus of the present invention, except initial concentration is carried out to high-salt wastewater using aerial cooler, waste water evaporation load is reduced Outside steam consumption quantity, its exterior thermal source uses low-pressure residual heat steam, cheap, while uses multiple-effect negative pressure evaporation, reduces Steam consumption quantity.About 320-340 kilograms/m of the total steam consumption quantity of system3Waste water, save very much.

Claims (3)

1. one kind contains Na+、K+、NH4 +、Cl-、SO4 2-、NO3 -The highly concentrated effluent brine method of comprehensive utilization of coal chemical industry, it is characterised in that: Comprise the steps:
(1) hardness is removed:PH value 10.5-11 highly concentrated effluent brine (abbreviation high-salt wastewater, similarly hereinafter) is pumped into softening depositing reservoir first, The liquid caustic soda for adding mass concentration 42-50% adjusts pH value to 11.5-12, makes the Mg in waste water2+Sunk in the form of magnesium hydroxide Get off in shallow lake;Then sodium carbonate is added, by Ca in water2+Content, add 1-1.5 kilograms per square waste water, purity is more than 98%, makes Ca2+Precipitate as calcium carbonate;To make precipitation abundant, agitator is slowly stirred by the 50-60 per minute speed turned in pond Mix;During magnesium hydrate precipitate, silica can precipitate a part therewith, so as to reduce the concentration of silica in water;Pass through slag Stock pump, from softening depositing reservoir bottom collection precipitating sludge, is discharged into the existing sludge collecting pit of enterprise, with original at interval of 48-72 hours The sludge mixing come;Mixing sludge is dehydrated to solid content in 30-40% through centrifugal dehydrator, by transported on trucks to Treatment of Sludge factory Disposal;
(2) one-level coagulating sedimentation tentatively removes COD:To remove up to 600-1000mg/L COD in highly concentrated effluent brine, acid is taken The technique of property coagulation is degraded:Softening depositing reservoir supernatant overflow enters one-level coagulative precipitation tank, is connected by acid adding measuring pump The continuous hydrochloric acid by mass concentration 25-31% is added in pond and stirred, and pH value is adjusted to 2-3, makes calcium, the magnesium remained in supernatant Ion is dissolved into water in the form of calcium chloride, magnesium chloride;Coagulation occurs for Organic substance in water simultaneously, adds poly-ferric chloride to flocculate Agent, per square 20-50 grams of waste water dosage, be allowed to further flocculation sediment, the organic particle to precipitate through Pulp pump at interval of 48-72 hours squeeze into the existing sludge collecting pit of enterprise, with original sludge mixed processing;The supernatant overflowed is beaten through pump Enter filter to be filtered, the high-salt wastewater after filtering enters high-salt wastewater primary concentration system buffer pool by overbottom pressure, filters out The impurity come is periodically discharged into the existing sludge collecting pit of enterprise;COD contents are down to 350-450mg/L after one-level coagulating sedimentation;
(3) high-salt wastewater primary concentration:Added into buffer pool mass concentration 42-50% liquid caustic soda by pH value of waste water adjust to 6.5-7, then boosted pump squeeze into primary concentration system air cooler, flowed from top to bottom after cloth liquid;Extraneous air passes through Air blower introduces aerial cooler, is flowed from bottom to top through subcooler inner stuffing;Air-liquid two-phase countercurrently connects between filler Touching, the clean moisture in high-salt wastewater constantly evaporates to be shifted into air, when air is reached at the top of aerial cooler, water therein Steam reaches saturation partial pressure, and mass concentration 15-20% moisture is got into the air in the form of saturated steam in high-salt wastewater, Unsaturated air is changed into saturated air, after aerial cooler epimere dehydrater further removes aqueous water, arranged from top Enter in air, high-salt wastewater is obtained initial concentration, so as to save the cost of later stage concentration;By the high-salt wastewater weight of initial concentration Newly it is discharged into primary concentration system buffer pool, carries out circulation concentration;
(4) high-salt wastewater secondary concentration:The high-salt wastewater for obtaining initial concentration squeezes into waste water secondary concentration through pump from buffer pool The evaporator of system, by the way of multiple-effect evaporation concentration, heated with external 0.4-0.6MPa low pressure saturated steam, in 55- 120 DEG C, by Waste water concentrating to sodium chloride therein close to saturation;Evaporation condensed water and water vapor condensation water are from secondary concentration system Discharge, respectively enters evaporative condenser water pot and steam condensate (SC) tank is standby;Concentrated mother liquor is discharged into two-stage coagulation sedimentation basin;
(5) two-stage coagulation precipitation removes COD again:In high-salt wastewater after I and II concentrates, COD contents are concentrated into 6000-6500mg/L, the technique of secondary acid coagulation is taken further to degrade:High-salt wastewater concentrated mother liquor pump after secondary concentration Enter two-stage coagulation sedimentation basin, continuously mass concentration 25-31% hydrochloric acid is added in pond and stirred by acid adding measuring pump, by pH Value regulation makes the Ca remained in mother liquor to 2-32+、Mg2+Ion is dissolved into water in the form of calcium chloride, magnesium chloride;Water simultaneously Middle organic matter, coagulation occurs, adds poly ferric chloride flocculant agent, per square 20-50 grams of waste water dosage, be allowed to further flocculation sediment, The organic particle to precipitate squeezes into the existing sludge collecting pit of enterprise through Pulp pump at interval of 48-72 hours, and original Sludge mixed processing;The supernatant overflowed is squeezed into filter through pump and filtered;Mother liquor after filtering is squeezed into plus alkali pond, throws Mass concentration 42-50% liquid caustic soda is added to adjust pH value to 6-7, the supernatant overflowed squeezes into filter mistake again through pump Filter;High-salt wastewater after secondary filter enters high-salt wastewater three-level concentration systems by overbottom pressure;Two-stage coagulation sedimentation basin plus alkali bottom of pond Portion's mud and the impurity filtered out are periodically discharged into the existing sludge collecting pit of enterprise;The COD contents after two-stage coagulation precipitates It is down to 1000-1500mg/L;
(6) waste water three-level concentration and recovery anhydrous sodium sulfate:Salt-mixture mother liquor after two-stage coagulation precipitates and filters, is squeezed into through pump Waste water three-level concentration systems evaporator, the mode of evaporation and concentration is taken, between 70-75 DEG C, by Waste water concentrating to sulfuric acid therein Potassium, so that the sodium chloride, sodium sulphate mass crystallization in waste water separate out, through further stiff, enters close to saturation into centrifuge Row first-stage centrifugal separates;Sodium sulphate, the sodium chloride mixture isolated add the evaporation condensed water of secondary concentration system, in 70- 75 DEG C sodium chloride therein is completely dissolved after carry out two-stage centrifugal separation;The sodium sulphate centrifuged out adds secondary concentration system The evaporation condensed water of system, is washed at 70-75 DEG C, and sodium chloride therein is completely dissolved, and then carries out three-level centrifugation, The anhydrous sodium sulfate of high-purity is obtained, entering warehouse after the processing of dry packing system sell;The mother liquor of first-stage centrifugal separation is pumped into Salt-mixture system for concentrating and recycling, the mother liquor of two-stage centrifugal separation are pumped into sodium chloride, sulfuric acid mother liquid of sodium freezing and crystallizing system;Three-level from Heart separating, washing liquid squeezes into sal glauberi evaporator;Three-level concentration does thermal source using indirect steam caused by secondary concentration, no The outer next life steam of consumption, it is standby that evaporation condensed water is discharged into evaporative condenser water pot;
(7) sodium chloride, sulfuric acid mother liquid of sodium freezing and crystallizing reclaim sodium sulphate again:The separation of waste water three-level concentration systems two-stage centrifugal To -5-0 DEG C, sal glauberi mass crystallization separates out for sodium chloride, sulfuric acid mother liquid of sodium frozen cooling, after first-stage centrifugal separation, adds Evaporation condensed water dissolves, and three-level concentration systems are drained through the three-level centrifugation sodium sulphate cleaning solution come and enter ten water sulfuric acid together Sodium evaporator, thermal source is done using indirect steam caused by secondary concentration, concentration is evaporated at 70-75 DEG C, anhydrous sodium sulfate is big Amount crystallization is separated out, and two-stage centrifugal separation is carried out into centrifuge;Solid sodium sulfate after centrifugation is sent into three-level concentration systems, The sodium sulphate separated with three-level concentration systems two-stage centrifugal washs recovery in the lump;Mother liquor after sal glauberi centrifugation It is pumped into salt-mixture system for concentrating and recycling;It is standby that evaporation condensed water is discharged into evaporative condenser water pot;The sulfuric acid reclaimed through step (6)-(7) After sodium mixing, by mass percentage, sodium sulphate purity 98-99.13%, the rate of recovery is more than 98%, and sodium chloride content is no more than 1%, nitric acid sodium content is no more than 0.4%, and sulfuric acid potassium content is no more than 0.1%;
(8) sodium chloride mother liquor concentrations recovery sodium chloride:Sal glauberi centrifuges mother liquor and is pumped into sodium chloride evaporator, by 0.4- 0.6MPa external vapor heat supply, solution is evaporated to supersaturation at 100-120 DEG C, sodium chloride mass crystallization separates out, through thick Thickness, first-stage centrifugal separation is carried out into centrifuge;The sodium chloride centrifuged out adds the evaporation condensed water of secondary concentration system, Washed at 70-75 DEG C, sodium sulphate therein, potassium sulfate, sodium nitrate be completely dissolved, then carry out two-stage centrifugal separation, The sodium chloride of high-purity is obtained, entering warehouse after the processing of dry packing system sell;One-level, the mother liquor mixing of two-stage centrifugal separation Afterwards, mass concentration 80-85% squeezes into sodium chloride, sulfuric acid mother liquid of sodium freezing and crystallizing system circulation freezing and crystallizing sal glauberi, matter Amount concentration 15-20% is pumped into salt-mixture system for concentrating and recycling;It is standby that steam condensate (SC) is discharged into steam condensate (SC) tank;Steam condensate (SC) It is standby to be discharged into steam condensate (SC) tank;In the sodium chloride of recovery, by mass percentage, sodium chloride purity 98-99.13%, the rate of recovery 88-90.77%, sodium sulphate content are no more than 0.5%, and nitric acid sodium content is no more than 0.5%, and sulfuric acid potassium content is no more than 0.2%;
(9) salt-mixture concentration and recovery:Mother liquor, sal glauberi after the separation of waste water three-level concentration systems sodium sulphate first-stage centrifugal steam The mother liquor after device evaporation and two-stage centrifugal separation is sent out, after being mixed into salt-mixture concentration systems, salt-mixture concentration systems is pumped into and enters Row is concentrated by evaporation, and thermal source, between 60-90 DEG C, 3K are used as by the use of the indirect steam of sodium chloride system for concentrating and recycling2SO4· Na2SO4、NaNO3·Na2SO4、NaNO3、(NH4)2SO4Salt-mixture mass crystallization separates out, and is centrifuged through stiff into centrifuge Separation;The solid salt-mixture moisture content mass percent centrifuged out be no more than 5%, it is packaged after directly as agricultural mixing Chemical fertilizer is sold;Mass concentration 80-85% mother liquors after centrifugation squeeze into the crystallization of salt-mixture system for concentrating and recycling circulating and evaporating, matter Amount concentration 15-20% squeezes into the original sludge treatment pond of enterprise, is handled together with other impurities sludge;Evaporation condensed water is discharged into steaming It is standby to send out condensate water pot;The salt-mixture of recovery, by mass percentage, nitric acid sodium content 50-60.03%, potassium sulfate contain in butt 15.5-20.55% is measured, sodium sulphate content is no more than 5%, ammonium sulphate content 8.3-12.1%, sodium chloride content 5.7-9.47%, Other impurities are no more than 4%;
(10) recovered steam condensed water and evaporation condensed water:The remaining evaporation condensed water of evaporative condenser water pot, directly returned by enterprise With production system, rate of recovery 90-93%;Residual steam condensed water is by enterprise's direct reuse steam generator system, rate of recovery 95-97%.
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